US1774410A - Process of precipitating boron - Google Patents

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6, 1930. A. E. VAN ARKEL 1,774,410

PROCESS OF PRECIPITATING BORON Filed Aug. 18, 1926 Patented Aug. 26, 1930 V UNITED STATES PATENT OFFICE ANTON EDUARI) VAN ABKEL, OF EINDHOVEN, NETHERLANDS, ASSIGNOR TO N; V. PHILIPS GLOEILAMPENFABRIEKEN, OF EINDHOVEN, NETHERLANDS PROCESS OF PRECIPITATING BOB ON Application filed August 18, 1926, Serial No. 130,083, and in the Netherlands October 5, 1925.

The present invention is concerned with a process of precipitating boron and has for its object to precipitate boron in a coherent form. It has been proposed to precipitate boron from boron halid on an incandescent surface reducing the halid by means of a reducing gas, such as hydrogen. The present method of precipitating boron in a coherent form on a body having a sufficiently high melting point, consists in heating the body in an atmosphere of one or more of the halogenides of boron, without making use of any reducing agent. Preferably, said body should be heated in an atmosphere of boron bromide. Owing to the high temperature to which the core is heated the boron halide dissociates whereby boron deposits on the core in a coherent form and the halogen is liberated. According to the, invention this halogen can be removed by introducing into the reaction vessel a substance which chemically binds the halogen. For this purpose mercury should preferably be used, in which case the halogen is bound as a mercury halide. In order to precipitate boron in accordance with this process, it suflices that the atmosphere exclusively consists of one or more halides of boron. Although the presence of some admixtures will not exercise any detrimental influence on the favourable course of the boron precipitation, there are admixtures which have an unfavourable influence on the course of the process and which even are able to prevent the precipitation of boron as such. Thus, for example, it has been found that a slight addition of nitrogen gives rise to the formation of boron nitride and that an addition of hydrogen causes the boron to precipitate in a non-coherent form.

The process will be elucidated by an example which will be described with reference to the drawing accompanying the present specification. In this drawing the numeral 1 refers to a glass vessel in which at 2 and 3 leading-in wires for an electric current are sealed. In this vessel a tungsten Wire 7 is fixed to said two leading-in wires. To the bottom of the vessel 1 are sealed two small vessels 4 and 5 which are destined to contain boron halide. At 6 a quantity of mercury tric current to a temperature of about 1400 Q, the vessel 5 which when starting is empty is cooled for example with the aid of liquid air and the vessel 4 filled for example with boron bromide is maintained room temperature is sufliciently volatile, will evaporate and when touching the filament will be dissociated whereby boron recipitates on the wire and bromine is li erated. The bromine will be bound by the mercury present at 6. The boron bromide which has not been dissociated, is condensed in the vessel 5. Owing to the evaporation of the boron bromide in the vessel 4, the latter will be cooled to a. tcmperaturelying below room temperature. It is therefore advisable to heat the vessel 4 to such an extent that the boron bromide always remains at room. temperature. When all the boron bromide ofv the vessel 4 has been evaporated, the heating device may be transferred from the vessel 4 to the vessel 5 in which a certaln quantity of boron bromide has assembled whereupon the vessel 4 may be cooled with the aid of liquid air. tinued whilst interchanging each time the functions of the vessels 4 and 5. By this process the boron precipitates on the tungsten wire as a firmly coherent layer. It is obvious that the current which originally is sent through the tungsten wire, must be raised as the wire grows in size lest the temperature of the wire should fall during the reaction. It has been found that this does not cause any difliculties because the resistance of boron which at a low temperature is very high, is low at the reaction temperature.

Boron can be precipitated not only on tungsten but also on other materials and even on boron itself, which practically happens as soon as the core wire has been coated with a layer of boron. If it is desired to produce very thick boron wires or rods, it is advisable to carry out the process in several stages, for

example in several reaction vessels and to at room temperature. Now the boron bromide which at 60 This may be con- 80 choose each time the thickness of the leadingin wires with regard to the thickness of the boron wire. In order to cause a boron wire to glow, the latter must first be brou ht up to incandescence with the aid of a hig 1 tension. Thus, for example, a boron wire having a thickness of 1 mm. and a length of 5 cm., needs a tension of 3000 volts in order to arrive at incaudescence. This tension should be decreased in proportion as the temperature of the wire increases and at 1000 C. the resistance is about one million times smaller that at room temperature.

Owing to its property of having a high resistance at a low temperature boron in a coherent form may be used as a resistance material. Boron in a coherent form further proves to be an excessively hard material which as regards hardness lies between corundum and diamond.

What I claim is 1. The process of precipitating boronin a coherent mass on a body having a high melting point, comprising, arranging a body which is chemically inert toward a halide of boron, in an atmosphere of at least one of the halides of boron, and raising the body to a temperature sulficiently elevated to cause disassociation of the halide of boron in the said atmosphere solely by heat, thereby causcausin it to combine chemically with a suitable su stance.

5. The process of precipitating boron in a coherent mass on a body having a high melting point, comprising, arranging a body which is chemically inert toward a halide of boron, in an atmosphere of at least one of the halides of boron, raising the body to a temperature sufficiently elevated to cause disassociation of the halide of boron in the said atmosphere solely by heat, thereby causing the deposit of the boron on said body, and concurrently clearing the atmosphere of the bromide freed by the said disassociation, by combining it chemically with mercury.

In testimony whereof I aifix my signature, at the city of Eindhoven, this 4th day of August, A. D. 1926.

ANTON EDUARD VAN ARKEL.

in an atmosphere of boron bromide, and

raising the body to a temperature sufficiently elevated to cause disassociation of the boron bromide in said atmosphere solely by heat, thereby causing the deposit of the freed boron on said body.

3. The process of precipitating boron in a coherent mass on a body having a high melt- .ing point, comprising, arranging a body which is chemically inert toward a halide of boron, in an atmosphere of at least one of the halides of boron, raising the body to a temperature sufiiciently elevated to cause disassociation of the halide of boron in the said atmosphere solely by heat, thereby causin the deposit of the boron on said body, an concurrently clearing the atmosphere of the bromide freed by the said disassociation.

4. The process of precipitating boron in a coherent mass on a body having a high melting point, comprising, arranging a body which is chemically inert toward a halide of boron, in an atmosphere of at least one of the halides of boron, raising the body to a temperature sufliciently elevated to cause disassociation of the halide-of boron in the said atmosphere solely-by heat, thereby'eausing the deposit of the boron on said body, and

concurrently'clearing the atmosphere of the bromide freed by the said disassociation by

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